Ethyl diazoacetate → Ethyl 2-chloro-2-fluorocyclopropanecarboxylate

HRID 468893노트

반응식

HRID 468893 반응식
[Cl:1][C:2]([F:4])=[CH2:3].[N+](=[CH:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[N-]>ClCCl>[Cl:1][C:2]1([F:4])[CH2:3][CH:7]1[C:8]([O:10][CH2:11][CH3:12])=[O:9]

참가 물질

4

반응물 2

HCID 12192Ethyl diazoacetateHCID 753441-Chloro-1-fluoroethene

생성물 1

HCID 9793930Ethyl 2-chloro-2-fluorocyclopropanecarboxylate수율 76%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a suspension of tetrakis(triphenylacetate)dirhodium (3.66 g) and powdered molecule sieves (45 g) in dichloromethane (2.0 L) was added 1-chloro-1-fluoroethene (82 g, 1.02 mol) at −60° C. The reaction mixture was warmed to −35˜−40° C., ethyl 2-diazoacetate (90 g, 790 mmol) in DCM (200 mL) was added and the reaction mixture was stirred at room temperature overnight. The reaction mixture was filtered and evaporated in vacuo to yield 100 g Ethyl 2-chloro-2-fluorocyclopropanecarboxylate as yellow oil which was used directly in the next step without purification.

후처리

  1. temperatureThe reaction mixture was warmed to −35˜−40° C.
  2. filtrationThe reaction mixture was filtered
  3. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-90142c9aad19424c8b03237cfe4a2951
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623889B2

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